The Chemical characterisation of E-device Aerosols
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1 The Chemical characterisation of E-device Aerosols Stuart Martin & Chris Rawlinson CORESTA SSPT ST02 30 th September 2013 Group R&D, British American Tobacco, Southampton, UK
2 Introduction BAT s initial approach to chemical characterisation Limitations to recent approach Device sampling considerations Ideal world for sampling and analysis - Environment - Sampling equipment - Method of collection Aerosol assessment by TD-GC-TOFMS Evolution of terminology/nomenclature Summary Acknowledgements Questions 2
3 BAT s initial approach to chemical characterisation of e-devices E-device aerosol The combustible approach filter pad collection + bag collection Figures courtesy of Justin Frosina & Jason Adamson
4 BAT s initial approach to chemical characterisation of e-devices E-device sampled on smoke machine 80/3/30) Tedlar bag Cambridge filter pad (CFP) Gas analysis Add benzene-d6 Mixed Injected onto cryocooled GC-MS via 2mL sample loop Analysed scan mode (25-250amu) Headspace analysis ¼ CFP add 20ug toluene-d 8 Analysed by SPME-GC-MS (29-400amu) Liquid injection ¾ CFP add 200ug toluene-d 8 Extracted 15mL methanol Analysed by liquid injection GC-MS (29-400amu)
5 Limitations to initial approach: vapour phase analysis and CFP solvent extracts Vapour Phase Large dilution effect = limited sensitivity: - LOD benzene-d6 ~0.1µg/L (S/N 10:1) - LOD acetaldehyde ~7.9µg/L (S/N 10:1) - Some volatiles may be retained on bag CFP solvent extracts CFP in 15mL methanol = dilution effect Limited sample information Abundance 1e ethanol benzene-d glycerol TIC: D nicotine menthol Only 8 samples/day: - Tedlar bags analysed within 15 minutes - CFP preparation time Time-->
6 Limitations to recent approach: Headspace-SPME min per sample ~50-60 components detected (Inc. artifacts) Useful information after 22 mins 1-2 hours manual data processing time 8 samples/day
7 Device sampling considerations Smoke machine cross-contamination from combustible products: Abundance TIC: _02.D benzene-d6 Abundance toluene TIC: _02.D\data.ms TIC: _03.D\data.ms (*) TIC: _04.D\data.ms (*) TIC: _05.D\data.ms (*) TIC: _06.D\data.ms (*) TIC: _07.D\data.ms (*) TIC: _08.D\data.ms (*) toluene Volatiles persist after 6 samples isoprene acetone Time--> Time-->
8 Device sampling considerations Need to consider choice of smoking machine: - Flow path complex in rotary machines = carry-over Abundance 1.1e+08 T IC: D \ data.ms T IC: D \ data.ms (*) T IC: D \ data.ms (*) 1e+08 9e+07 8e+07 7e Air blank after E-cig 6e+07 5e+07 4e E-cig sample 3e+07 2e+07 Time--> 1e Air blank CFP Lessons learned: - More sensitive analytical techniques required (esp. for gases) - Segregate combustible and non-combustible sampling; Effective cleaning - Choice of smoking machine and optimised flow path
9 E-device chemical assessment Are existing analytical smoke methods suitable for assessing e-devices? - YES: for bulk components (nicotine, PG, glycerol, water) - NO: for qualitative screening E-devices are not cigarettes - Sampling: background contamination of sample - Collection: e-device aerosol different from smoke - Analysis: less complex profile; most constituents at low levels Figures courtesy of Ross Cabot
10 Ideal world for sampling and analysis Environment Smoke and contaminant free Define suitable cleaning procedures and cleaning agents Assess the background regularly Equipment and Sample collection Minimum flow path in collection system Clean and inert surfaces (e.g. steel, Teflon, glass) Easy to clean Flexible to different collection systems (sorbent tubes, CFPs, impingers, bags) Variable puff volumes Repeatable Chemical analysis Sensitive (minimise dilution, maximise instrument sensitivity) Robust and repeatable between analysts Fast analysis time Reliable automated data processing (requires optimised chromatography))
11 Whole aerosol assessment by TD-GC-TOFMS E-device aerosol (whole) TD Tube Tenax TA / SulfiCarb TD- TOF MS 11
12 TD-GC-TOFMS: aerosol sampling Producing and capturing whole aerosol Manual Air Sampler Markes International Easy-VOC Borgwaldt A14 syringe drive Vs. Zero dead volume connection using Tygon tubing 12
13 Comparing air sampling methods 2-Propen-1-ol Nicotine Based on 5 replicates A14 shows higher precision
14 TD-GC-TOFMS: Analysis Summary A14 Syringe drive - Consistent delivery - Flexible collection system Whole aerosol captured by TD tube - Single analysis - Solvent free extraction - Concentration step - TD tubes can be reconditioned A single 25mL puff over 2s - Fast sample generation - No dilution effect Analysed by TD-GC-TOFMS - Quick and sensitive Data interpretation - Automatic deconvolution software Almsco TOF-MS Agilent GC Markes TD 14
15 TD-GC-TOFMS whole aerosol screen of E-cig 1 x 25mL puff / 2 seconds ~130 components detected <20 min analysis time 10 min data processing 100 samples/day 15
16 TD-GC-TOFMS whole aerosol screen Meeting the challenge of sensitivity E-cig vapour (25mL puff) 5ng EPA 8260B VOC standard mix (split flow) 16
17 TD-GC-TOFMS whole aerosol screen Analytical challenges Peak overload nicotine Heart-cut glycerol to FID Protect MS detector glycerol propylene glycol 2-propen-1-ol 17
18 Summary Existing Methodology New Methodology ~50-60 Components Detected ~130 Components Detected 1 hour Analysis Vs.. <20 min Analysis 1 hour Data Process 10 min Data Process 0.1µg (1µg/L) LOD <5ng LOD (on tube) 8 Samples/day 100 Samples/day 18
19 Summary Existing Methodology New Methodology ~50-60 Components Detected 1 hour Analysis Smoke methodology not appropriate 3 GC-MS scan methods into 1 2 x more components detected Vs.. 20 x Increase in sensitivity 12 x Increase in throughput ~130 Components Detected 15 min Analysis 1 hour Data Process 10 min Data Process 0.1µg (1µg/L) LOD <5ng LOD (on tube) 8 Samples/day 100 Samples/day 19
20 Evolution of nomenclature Need to evolve a new set of terms to distinguish e-devices from combustible products: Vapour/particulate phase whole aerosol Device smoking device sampling TPM aerosol condensate?
21 Conclusions Applying smoke methodologies to E-devices is not always appropriate: - Sensitivity - Dilution effects - Contamination/carry-over issues Need to consider environment of sampling: - Effective management of background - Segregate from combustible analysis TD-GC-TOFMS is one alternative: - Sensitive - High throughput - Solvent free Evolution of appropriate terminology/nomenclature 21
22 Acknowledgements Colleagues at BAT Group R&D Pete Davis Trevor Enos Ross Cabot Justin Frosina Jason Adamson Chris Wright
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